Phosphorizing nozzle



Dec. 22, 3.953 J. R. WYATT 2,663,590

PHOSPHORIZING NOZZLE Original Filed May 16, 1947 4 Sheets-Sheet lINVENTOR IQI I II I {I I Il II IIII IIHIHI .MHV H. mmm! -m MIIII. QN

I wwwww I J. R. WYATT PHOSPHORIZING NOZZLE Dec. 22, 1953 4 Sheets-Sheet2 riginal Filed May 16, 1947 INVENTOR NM @v 4 Sheets-Sheet 1N ENToR YIlmlx.

ilrlll l El J. R. WYATT PHOSPHORIZING NOZZLE Dec. 22, 1953 originalFiled May 16, 1947 Dec. 22, 1953 J, R, WYATT 2,663,590

PHosPHoRIzING NozzLE original Filed May 16, 1947 y 4 sheets-sheet 4INVENTOR ORNEYS Patented Dec. 22, 1953 Eto :1 :My :inventien fmelates temapa/rams fer :nlxoiia phorizing and especasla,1 .Sfm :phosphor 'sappenA nventonifistbducetheia cident nate :and er vielixn'inmae V4mue ,gheamAl'rzmdinfp'lfmsphorizing.. v

farmer @purpose Vsis ttu :ieiimnate the smoke nuisance "finement stepresem methods of nanos- Uhriing. A further purp'oses wineresebhe :alsoincrease `he rate ef fphosphorus :absarpstinn by mixen meta-1 nt; yield.Pand vpermid', A further purpnse iis www copper mmsnhonasnefmnnasphorizing. f

eaka'g'e incident :to @hanging :phusphenus -metal fby vnf @phosphorus*va-per lmoceeding I have hesen to r11-Imate .inventin 44e @engin sw, be

.i faisais-ana endemica-mgm thefdrawings:

Widely known e meblevinnir im A i n ,e wnvertedfto ren-fphosrpherusfwhm@and Offlligher memngimi-n @heien-@123mm akingmhgspher meer has been @1w@wat when sphoepharus 15h a. protective layer of copper, and to cli-ergethe @newwiesi'eakesnfaunes@Gewinne-#hemmen cepnenmreenably belg /th ceof.thebai'h, lhisyhasheema ha ou Qcegpatiorysit'Ifnespmsentfinvenmrinasmerimemqedewimhgmis technique andmesig'nedamzapparam's 'fsfthis The :mbbrem huwevernismqt fsimpeis-v-ane'girammutiewexitiealfutenm 60.

3 almost inevitably some part of the retort or connections will operateat a temperature favoring the formation of red phosphorus, and at suchlocations red phosphorus accumulates rapidly, clogging the apparatus andnecessitating frequent shut-downs for cleaning. Since the apparatus isinitially thoroughly filled with phosphorus vapor, and white phosphorusis retained in many parts of the equipment, cleaning is a veryhazardous` occupation, and it becomes a question whether it is not saferto use the welll known practice of charging copper coated cakes of whitephosphorus. Added to this is the certaintythat any leakage of phosphorusvapor from the retort may have fatal consequences to workmen.

' Burns U. S. Patent No. 2,164,228 applies molten phosphorus to metal byan apparatus which is essentially a dropping funnel suspended above themolten metal bath, in which phosphorus is melted below water, and fromwhich it is dropped under valve control into a nozzle beneath thesurface of the metal. This presents the difficulty of exposing theentire mechanism to the heat of the molten metal bath, and hazardingdiiiculty or danger through leakage, since the dropping funnel must beopened periodically to introduce cakes o f white phosphorus.

' In accordance with the present invention, the difficulties of thevarious prior art `processes are overcome Without appreciable increasein the cost of the operation.

It has been foundthat by the present invention, the ,loss inphosphorizing copper can be cut to of the loss presently encountered incharging coppercoated cakes of white phosphorus', At

the same time the smoke nuisance is largely eliminated. vHandling ofthephosphorus by the individualworker can be entirely eliminated. Thestepof copper coating the phosphorus is rendered unnecessary. Theprocess is'made continuous, with'very excellent control over both thetotal amonut of phosphorus alloyed, and the rate of alloying. The speedof alloying Acan be increased beyond that at present practiced.

The hazard through accident or. impairment f health is practicallyeliminated, both from handling of phosphorus and from phosphorus moltenmetal, thus maintaining a temperature which will prevent formation of'red phosphorus.'

A Considering rstthe'formlof Figures l and 2, I provide atank'-conveniently open at thetop, andmade frornfa'ny'suitable materialsu'ch as steel or stainless steel, .The tank is lled to a convenientheightw'ith inert liquid 2|, suitably water. As the purpose of me inertiiquid-is partially -heat transfer, partially prevention of combustionof White phosphorus, and partially displacement of phosphorus, it willbe evident that water is the preferred inert liquid, but that othersuitable inert liquids may be used, as, for example, phosphoric acid or,where the rire hazard can be controlled, a mineral oil such as kerosene(kerosene is not recommended because of the fire 4 hazard). The tank231s heated by any suitable means, such as gas burner 22 having a gasconnection 23, an air inlet 24 and a combustion gas flue 25 suitablypassing up through the tank 20.

Within the tank 20, two pools of molten phosphorus 26 'and 21 arelocated, each having upon its surface a pool of inert liquid 28 or 29,which U will be desirably identical with the inert liquid 2 The pool ofmolten phosphorus 23 and of inert liquid 28 is contained within a tank30, and the pool of molten phosphorus 21 and of inert liquid 29 iscontained within the tank 3|. Both tanks are suitably of steel orstainless steel, in heat transfer relation with the tank 20, and thepool of inert liquid 2| contained therein. The tanks 30 .nad 3| maysuitably be supported on a frame 32 in the bottom of the tank 20.

Access to the interior of the tank 3| is not nec-` essary in theprocess, and one of the advantages of the process is the'fact that thehead 33 of tank 3| can be permanently gasketed'or welded on at 34 toprevent the possibility of leakage, andY particularly to prevent thepossibility of any escape of phosphorus vapor, if vapors should becarried back from the discharge nozzle.

On thev other hand, the head 35 of tank 30 is removably bolted andgasketed at 3S, so that it can be readily removed to introducewhitephos-V phorus to be melted in the pool 26. ,f

The melting tank 30 is connected through its head 35 to a source ofinert liquid under pressure; This is conveniently a pump 31 driven by amotor 38 having inlet at 39 from the pool 2| and discharging at 40through flexible connections controlled by valve 4|, the dischargepassin directly to the pool of inert liquid 28. A

The head 35 of tank 30 is also conveniently provided with a safety valve42.

To permit transfer of molten phosphorus from pool 26 to pool 21, aconnection 43 extends to near the bottom of pool 26 in tank 2D, throughunion 44 and valve 45 to pool 23 above pool21 in tank 3|. Tank 3| isequipped with mechanism 'to introduce a measured quantity of inertliquid into pool 29'. This is accomplished by pump 48 driven by motor 41having inlet at148 (desirably connected to the pool 2|, but broken awayto avoid compli-` cation in the drawing) and discharging throughconnection 49, relief valve Ell', pressure 'gauge 5|, ovv meter 52(rotating type) and flow meter 53 (variable orifice type), check valve54, and valve 55 to'the head 33 of tank 3|. An overflow valve to permitdischarge of inert liquid from pool 29 in tank 3| is provided at 5B.

As a means of checking the level of molten phosphorus in tank 3 I, oat5'! is provided in float column extending to the bottom of the moltenphosphorus, open at the bottom and closed at the sides, and havingindicator stem .59 in cover glass S0, closed at the top. Thecombinedweight of the float and indicator is chosen so that it is' lessthan the weight of the phosphorus displaced by the parts4 submerged inphosphorus, but greater than the weight oi the inert liquid'dis'- placedby the total submerged'parts if they were in inert liquid. All of thisof course presupposes the weight of the molten phosphorus and inertliquid at the particular temperature at which they are held. Thus thefloat will iioat on molten phosphorus but Will sink in inert liquid, theinert liquid being lighter than the molten phosphorus, and the positionof the iloatwill always indicate the top of the pool 21. Y.

From the dispensing pool 21, discharge is @C- complished to a dischargenozzle 6| below the $3 'bwa eomieetion .ol-extenong mathe .bettomfof thepooll'. t ismportan't f lihatithe @hose photos fshouii not solidifydiseueige een` neetion ano should not 4get :hot fito 'florian'hos'phorus lthere, :and ltlie'zefifie the disharge-uonnec on is'iaoketed preferably 'lby `"inthi -e'feifiquiufs tabry withdrawn-eh ai.,at the preferred temperature `fo about 1F30 "is jaeeonxpi'ishei bye pumpP65 driven 1by motor 165" fwhieh has E6 to ooi 2i fano isharges etfoi twater eeeketfee ingip'o'dl.

{forni 'o La eiose 'tank preferably 'ieitenufmg to a height'substantially above the-pools izo and The water column 1,5 is providedwith 'a 'liquid reve-1 ygauge We, suitably for the frsigni 'giass*familiar in boilers. 'fixiert fi'iquiu vvinlet "is proviued to theinert liquid column by a connectionlrom pump 'o1 feentroued'byveive "Hi'anu feonyeientiy entering y'near 'the l="c'lo'sed of the v"liquideoium'n.

scharge "of inert 1liquid afrom Ta 'point Auongiifgas *underpressuresuitably auen-compressor 'e2 .driven by 'motor te sito fdieerfargurgegimpressedsaiithroug'heonnectionsoarfdvivefoute .fm'il'guresienui'zftrre nozzle is df eonicalfiorm asimietertferomonas@coniearinteiofbore 8'1 est'ehiing *fromeuditoeuiiaertillyanueommunicating with connection 674. nozzle "is madeof suitable fmfractory material, preferably graphite.

InEig-ures and- 5 I rillustrateea variantform of nozzlel I which .is.suitably tubular in exterior dimension oontains *an interior 'conicalbore 81 enlarging from the inlet @to the outlet. Ellfe 'ole Bil "J'isEmosteonvenientty Fmanufaeturel by boring-@clit 2a graphite `electricfumnace il'eti'ode iothi siinilanoarbonrefraitoiyylinen whe -zle mountedYin a metalli@ '"nozzle 'flfrold'er 88 lfaing affsideopening'or nneciin'la `"'ur ea'ziladistanibi-itiony aainberilindfa ohaige 'foiioe 9|imfined 4`"l a'bove "loife B v'Illre "nozzle holder a ibiil'ar SoIQtZJQZiliieh'fifeeeives --the .opper ene fthe nozzieisft, makingvaporetightffseal bywa :fsteel bellows 93 betweenthe end of the nozzleand the base of the -sooktan'da packing 94fc`lanpe'd againstltlieiside"f "the 'nozzle "by 'a p'aking fing 95 `suitably threaded on the nozzleholder. The nozzle is held in the holder and drawn up tight against the'ieveifefitheimeneiiuieieifsz .im u einrumen-mueve 6 peeking :es:tyrants si eeungbetweeuiseuiai 91 Kentire holder 4mail vve. ysplit ringist attached im areeess 99-onfthemozzle iut :intervals around :thecircumference for nozzle abovetheaottom-.opening illl of thelbore, jetopenings 191 #are provided extending radially and preferablyy'fuorizmvarzily A"sin angle, as best seen Figure #L #It 'nos been roundin fan-'am tice that phosphorus drops through 'liche souifloe 9i, is-fexpeljleu im 'fiets through 'the e't epen'mgs 1 hi., eiftening forl-oonsiuerable fiietanees im the molten'-metailsuiwounuingtheprince,-anitnusibeeifeetivelyabso'rlbe. "Whenithe @volume-io? wapo' nteo great'to fisfiarge through fthe -tet operi-ings 1| nfl, "it is, -of :oeuf-se,Lfnfee ato discharge through the-fendfopemng flUll, @but :thepenetration 2nite 'the molten bath iis likely Vto be 7less fex ten'siveyand lozere -uepenienee placed upon fuir lus/ion fand istiring of 't'h'e'bath "to `obtaiizi 'orlnitydofphosphoizing l ftinasbeenteunu'iinfprafctiee with thei'etiofthe type of Figures 3, 4 and "n "abaffh'vfa'e quateesize toffmaiiitein itlife'v pre'ferablymitoot'erfmorebelow the fsurifaoet'hat there li'sne serious fianger of:phosphorus vapornot 1f-*being bsobeuibyftnenlten copper. ne anaoitionel promotion, ilrowever, against `this feentingency is desirableto carbon `Lon @the 'ibetn uit T82. aoni'rto Ynietinten an 'adequatesupply Yoi ein' soi'trrat ftnefcon'ditiorrs iee--oxiizii'lg above the n,aneanypossble @phosphorus schlug-ing fwour ipe #oxidized s"to finos--phorusfpentoxioe. "Tinsffeaturefisepreeeiutfonam, however, as `thesmallamourit eff smoke and -fyi'eliinuieateithit Tuttle T151iosplrorusfis fiest. itl-1e nozzle the holes iHH ima? `linge andthe @be 4lost, thevvapor:illzvafssfnxg' upward yalong the lfinitsiue surface of fthenozzle jinviti/rout r'tuiequraite feontaot with 1f/he 'meta-fl. -Iillustrate fan l:aumiliati" enlargement, ri'fin'g or shell 5I-'05a'fround tlre *nozle aboveithe openings IUI, which assures deflectionof'a`-1wil11`sh ifngwapor outwardly, and #adequatefefotact 'the'meltenim'tal Y v in making phosphor jcopper fthe -iopertion-dsusuanyeontintreu-.untl'- `"tout lires Menem biIred,thepercentagebeingsomewhat eritielifas j Iease fof nigheryril-respirorus eontents the illoy'fxnay {ke 1InfoperatonftheLapparati-xsfisfsetupastheigas-lorfotnerrulburnefbeingmntainediso thatthe #linertT-liuuitL'(Wae'r) TAixf'ill preferabiybefait ytltemperature 'of about 160 to 180F. in theipol If any mistake is made in charging by which 'pieces orfragments of phosphorus drop into the pool 2|, no serious harm is doneas the pool 2| provides protection from fire and the phosphorus will'simply remain at the bottom of the tank 2U, from which it may beremoved. l y In order to transfer phosphorus from pool 26 to pool 21,valve 45 in the connection 43 between the tanks and 3| is opened,overilow valve 56 on tank 3| is opened, and with pump 31 operating,valve4| is opened to apply inert 'liquid pressure to pool 28 on pool 26in tank 30. This results in forcing molten phosphorus from melting pool26 through connection 43 into tank 3|, where it drops into and formspart of dispensing pool 21. The level of molten phosphorus in pool 21 isshown at all times by float 51 on indicator 59, the molten phosphorus ofthe pool communicating with the float through the open bottom of column60. As soon as suiiicient phosphorus has arrived inpool 21, valves 4|,45 and 55 are closed and pump 31 is turned off.

In order to phosphorize, using the form of Figures 1 and 2, the nozzle6| is inserted well below the level of the molten metal in furnace 63,manipulating the nozzle by means of universal joint 13. Pump 64 isstarted so that the exposed portions of connection 64 are Well heated bythe warm inert liquid from pool 2|. To begin phosphorizing,pump 46 isstarted and valve 55 is opened to permit inert3liquid to enter pool28,and discharge valve 14 is opened to permit phosphorus to be displacedfrom pool 21 and discharge through the nozzle. Valves 55 and 14 areadjusted to obtain the desired flow as shown by flow meters 52'and 53.The quantity of phosphorus discharged by the nozzle can be determined,since it is equal to the quantity of inert liquid passing through theflow meters 52 and 53. The change in level of the noat 51 can be used asa check, and to be sure that the pool 21 is not completel The phosphorusdropping through the bore of the nozzle is very rapidly vaporized in-thenozzle and discharged as vapor into the molten metal. In most cases,molten-phosphorus never actually reaches the surface of the moltenmetal, but if it-does it is very rapidly vaporizedjand the vapor carriedinto the molten metal. Where a nozzle of the type of Figures 3, 4 and 5is used, this vaporization results in jets discharging through the jetopenings lill into the molten metal.

In the form of Figure 3, the pool 26 is lled as above described. Withall other valves closed, the air bleed 84' from the inertY liquid columnis opened. Pump 31 is started, and valve 13 opened to introduce inertliquid through connection 11 to a suitable level at the upper part ofthe gauge, if the inert liquid level be unduly low. Valves 18 and 84'are then closed. Pump 82 is started and valve 85 opened to apply airpressure to the top of the-inert liquid column, tending to force theinert liquid out of the column. Valve 88 is opened to connect the bottomof the inert liquid column with the pool 29 above the phosphorusdispensing pool 21. The nozzle 6| is suitably immersed well below thelevel of the molten metal 62 as shown in Figure 3, and the dispensingvalve 14 opened. Molten phosphorus from the pool 21 is now displacedthrough the connection 64 which is of course suitably heated by theheating jacket 68 supplied with 8 heated inert liquid through pump 65 aspreviously explained. The rate of dispensing of molten phosphorus can begauged by the W meter 8|, and the total quantity of phosphorus dischargecan be gauged by the difference in level ofv inert liquid on the gauge16, which will correspond with the volume of phosphorus dispensed. Thismethod of gauging is preferred because it is more accurate than the owmeter method.

It will be evident that by the present invention it is possible tointroduce phosphorus to a molten metal bath without handling of thematerial from the time it is first charged for melting, and even thiscan be done by handling a drum and without individual handling of cakes.It will further be evident that at the time that dispensing takes place,the connection to the melting pool through the valve 45 is closed, sothat the danger through leakage of the melting tankis avoidedl It willalso be evident that during dispensing, the molten phosphorus in thedispensing pool is protected not only by the pool of inert liquidcovering it, but also by the inert liquid being supplied from the pumpor from the inert liquid column.

In view of my invention and disclosure variations and modications tomeet individual whim or particular need will doubtless become evident toothers skilled in the art, to obtain all orpart of the benefits of myinvention without copying the apparatus shown, and I, therefore, claim'all such insofar as they fall Within the reasonable spirit and scope ofmy claim.

,Having thus described my invention what I claim as new and desire tosecure by Letters Patent is:

In a phosphorizing apparatus, a metering de-v vice dispensing moltenphosphorus at a controlled rate, a nozzle head connected with themetering device and having a-socket provided with an opening, a carbonrefractory nozzle element having a longitudinal bore tapering from asmaller cross section near an inlet end to a larger cross section nearan opposite outlet end, and having a ring of radial holes outwardly difrected from the bore to the outside nearvr the outlet end, the nozzleelement tting into the socket at the inlet end of the nozzle, a collarsurrounding and engaged-with the refractory, of the nozzle elementlocated at a positionl inter'- mediate between the inlet and outlet endsand screws extending longitudinally at spaced points around thecircumference and interconnecting the collar with the nozzle head.

JAMES R. WYATT.

References onse in the me of this patent UNITED sTATEs PATENTS Number vName Date 153,311 Bristol July 21, 1874 627,728 Gould June 27, 18991,423,650 Decuir July 25, 1922 1,612,456 Marron Dec; 28, 1926 1,644,290Titcomb et al Oct. 4, 1927 1,686,833 Moore Oct. 9, 1928. 1,803,425Cunningham May 5, 1931 1,832,873 Milner Nov. 24, 1931 1,837,339 SchlickDec. 22, 1931 FOREIGN PATENTS Number Country Date 106,956 switzerlandJan. 2, 1925

